β-谷甾醇与马来酸酐酯化产物的表征及高效液相色谱分析

Characterization and analysis by HPLC of the esterified product of β-sitosterol with maleic anhydride

应用差示扫描量热法、红外光谱法、核磁共振波谱法和高效液相色谱法对β-谷甾醇与马来酸酐的酯化产物进行了表征和分析.实验结果表明:β-谷甾醇与马来酸酐发生酯化反应,产物为β-谷甾醇马来酸单酯;用Hypers il ODS反相柱,以甲醇为流动相,在检测波长为210 nm、柱温为25℃、流速为0.7 mL.m i-n 1的实验条件下进行液相色谱分析,β-谷甾醇及其马来酸单酯能够达到基线分离,采用外标法对β-谷甾醇及其马来酸单酯进行了定量分析,相对误差在±5%之间.外标法测得β-谷甾醇及其马来酸单酯的回收率接近100%.

The esterified product of β-sitosterol with maleic anhydride was characterized and analyzed by DSC, IR, NMR and HPLC methods. The experimental results show that mono-β-sitosteryl maleate is the only esterified product of β-sitosterol with maleic anhydride. The β-sitiosterol and mono-β-sitosteryl maleate were analyzed using reverse-phase column Hypersil ODS with methanol as the mobile phase at 210 nm, 25 ℃ and flow rate 0.7 mL · min^-1. The β-sitosterol and the esterified product can be separated effectively and they can be quantitatively determined by the external standard method. Determined by the external standard method, the recoveries of β-sitosterol and mono-β-sitosteryl maleate were about 100% and the relative error was within ±5%.